公开(公告)号：US4973758A

公开(公告)日：1990-11-27

申请号：US439757

申请日：1989-11-21

申请人： Horst Behre ,  Lothar Jakob ,  Heinz U. Blank ,  Dietmar Mayer ,  Roland Busse

发明人： Horst Behre ,  Lothar Jakob ,  Heinz U. Blank ,  Dietmar Mayer ,  Roland Busse

IPC分类号： C07C37/04 ,  C07C39/14 ,  C07C209/18 ,  C07C211/57 ,  C07C211/58

CPC分类号： C07C37/04 ,  C07C209/18 ,  C07C211/58

摘要： The characteristic of the improved process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene is to carry out the alkaline pressure hydrolysis of the disodium salt of naphthalene-1,5-disulphonic acid at temperatures from 270.degree. to 290.degree. C. and under 14 to 20 bar using an excess of sodium hydroxide solution such that the molar ratio NaOH/disodium salt of naphthalenesulphonic acid is at least 12:1. The 1,5-dihydroxynaphthalene which is obtained in this manner, without hazard and in substantially higher purity, is then aminated with ammonia in the presence of ammonium bisulphite to give 1,5-diaminonaphthalene, it being possible to achieve a further increase in the degree of purity of the 1,5-diaminonaphthalene by increasing the molar ratio NH.sub.3 /1,5-dihydroxynaphthalene to at least 6:1.

摘要翻译： 制备1,5-二羟基萘和1,5-二氨基萘的改进方法的特点是在270〜290℃的温度下进行萘-1,5-二磺酸二钠盐的碱性水解 并使用过量的氢氧化钠溶液使14至20巴，使得萘磺酸的NaOH /二钠盐的摩尔比至少为12:1。 然后用亚硫酸铵存在下用氨将胺化得到的1,5-二羟基萘没有危害并且纯度高得多，得到1,5-二氨基萘，可以进一步增加 通过将NH 3 / 1,5-二羟基萘的摩尔比提高到至少6:1，1,5-二氨基萘的纯度。

公开(公告)号：US4705652A

公开(公告)日：1987-11-10

申请号：US867111

申请日：1986-05-23

申请人： Erich Hammerschmidt ,  Horst Behre ,  Heinz U. Blank ,  Dietmar Mayer

发明人： Erich Hammerschmidt ,  Horst Behre ,  Heinz U. Blank ,  Dietmar Mayer

IPC分类号： C07C301/00 ,  C07C67/00 ,  C07C271/10 ,  C07C309/43 ,  C07C143/30

CPC分类号： C07C309/43

摘要： Solid crystalline tetra-alkali metal salts of chromotropic acid, a process for their isolation and their use for the preparation of pure chromotropic acid or di-alkali metal salts of chromotropic acid.

摘要翻译： 变色酸的固体结晶四碱金属盐，它们的分离方法及其用于制备变色酸的纯变酸或二碱金属盐的用途。

公开(公告)号：US4338261A

公开(公告)日：1982-07-06

申请号：US247416

申请日：1981-03-25

申请人： Heinz U. Blank ,  Horst Behre ,  Hans W. Linden ,  Werner Mentzel

发明人： Heinz U. Blank ,  Horst Behre ,  Hans W. Linden ,  Werner Mentzel

IPC分类号： C07C309/47 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C143/60

CPC分类号： C07C303/06

摘要： Improved process for the preparation of 1-naphthylamine-4,6-disulphonic acid wherein the sulphonation of the 1-naphthylamine-6-sulphonic acid is carried out by adding the oleum at a temperature of 10.degree. to 70.degree. C., either to initially introduce sulphuric acid simultaneously with the 1-naphthylamine-6-sulphonic acid or to 1-naphthylamine-6-sulphonic acid, which is dissolved or suspended in sulphuric acid, and by using such a molar ratio of sulphur trioxide to 1-naphthylamine-6-sulphonic acid that 1.2 to 3 mols of sulphur trioxide are present per mol of 1-naphthylamine-6-sulphonic acid. The sulphonation mixture formed in the preparation can be sulphonated in a second sulphonation stage to 1-naphthylamine-2,4,6-trisulphonic acid.

摘要翻译： 制备1-萘胺-4,6-二磺酸的改进方法，其中1-萘胺-6-磺酸的磺化是通过在10℃至70℃的温度下加入发烟硫酸来进行的， 最初与1-萘胺-6-磺酸或溶解或悬浮在硫酸中的1-萘胺-6-磺酸同时引入硫酸，并且通过使用三氧化硫与1-萘胺-6-磺酸的摩尔比， 6-磺酸，每摩尔1-萘胺-6-磺酸存在1.2〜3摩尔三氧化硫。 在制备中形成的磺化混合物可以在第二个磺化阶段中磺化成1-萘胺-2,4,6-三磺酸。

公开(公告)号：US4426334A

公开(公告)日：1984-01-17

申请号：US368194

申请日：1982-04-14

申请人： Horst Behre ,  Heinz U. Blank ,  Otto Lindner ,  Willi Schossler

发明人： Horst Behre ,  Heinz U. Blank ,  Otto Lindner ,  Willi Schossler

IPC分类号： C07C309/50 ,  C07C67/00 ,  C07C301/00 ,  C07C303/44 ,  C09B29/30 ,  C07C143/48

CPC分类号： C07C303/44

摘要： The invention relates to a process for isolating H acid and K acid in the form of their monoalkali metal salts from acid aqueous solutions which contain these two acids and alkali metal ions and may contain other aminonaphtholdisulphonic acids, in which process H acid monoalkali metal salts are precipitated at elevated temperatures from solutions which contain not only sodium ions but also potassium ions and then precipitating K acid monoalkali metal salts by cooling down the filtrate obtained after separating off the H acid monoalkali metal salts.

摘要翻译： 本发明涉及一种从含有这两种酸和碱金属离子的酸性水溶液中分离其单碱金属盐形式的H酸和K酸的方法，并且可以含有其它氨基十氢四氢呋喃磺酸，其中H酸单碱金属盐为 在不仅含钠离子和钾离子的溶液中在高温下沉淀，然后通过冷却分离H酸单碱金属盐后得到的滤液而沉淀K酸单碱金属盐。

公开(公告)号：US4540817A

公开(公告)日：1985-09-10

申请号：US516438

申请日：1983-07-25

申请人： Horst Behre ,  Heinz U. Blank ,  Alfred Seyberlich ,  Ferdinand Hagedorn

发明人： Horst Behre ,  Heinz U. Blank ,  Alfred Seyberlich ,  Ferdinand Hagedorn

IPC分类号： C07B61/00 ,  B01J23/00 ,  B01J23/70 ,  C07C67/00 ,  C07C231/00 ,  C07C231/12 ,  C07C231/24 ,  C07C233/43 ,  C07C102/00

CPC分类号： C07C231/12

摘要： A process for the preparation of 5-amino-2,4-dimethylacetanilide by reduction of 5-nitro-2,4-dimethylacetanilide with hydrogen is disclosed characterized in that a crude mixture containing 5-nitro-2,4-dimethylacetanilide in admixture with at least one of its position isomers is hydrogenated in a water-miscible organic solvent which optionally contains water. The 5-amino-2,4-dimethylacetanilide is separated off from the reaction mixture by means of crystallization employing a mixture of water-miscible organic solvent and water.

摘要翻译： 公开了通过用氢还原5-硝基-2,4-二甲基乙酰苯胺制备5-氨基-2,4-二甲基乙酰苯胺的方法，其特征在于将含有5-硝基-2,4-二甲基乙酰苯胺的粗混合物与 其至少一种位置异构体在任选含有水的水混溶性有机溶剂中氢化。 通过使用水混溶性有机溶剂和水的混合物的结晶从反应混合物中分离出5-氨基-2,4-二甲基乙酰苯胺。

公开(公告)号：US4407762A

公开(公告)日：1983-10-04

申请号：US410746

申请日：1982-08-23

申请人： Heinz U. Blank ,  Horst Behre ,  Hans W. Linden ,  Werner Mentzel

发明人： Heinz U. Blank ,  Horst Behre ,  Hans W. Linden ,  Werner Mentzel

IPC分类号： C07C309/47 ,  C07C67/00 ,  C07C301/00 ,  C07C303/44 ,  C07C143/60

CPC分类号： C07C303/44

摘要： Process for the isolation of 1-naphthylamine-4,8-disulphonic acid from sulphonation mixtures containing it according to which process the sulphonation mixture is introduced into preheated water in such a manner that, at the start of crystallization, a temperature of at least 100.degree. C. is reached and the 1-naphthylamine-4,8-disulphonic acid is separated from the mother liquor at a temperature not higher than 70.degree. C. The process is applied particularly advantageously for the isolation of 1-naphthylamine-4,8-disulphonic acid from sulphonation mixtures which have been obtained by introducing in turns alkali metal sulphate, 1-naphthylamine-8-sulphonic acid and SO.sub.3 into sulphuric acid which has been introduced initially, a total of 1.5 to 3 mols of SO.sub.3 and 0.6 to 1.5 mols of alkali metal sulphate being employed per mol of 1-naphthylamine-8-sulphonic acid.

摘要翻译： 从含有它的磺化混合物中分离出1-萘胺-4,8-​​二磺酸的方法，根据该方法，将磺化混合物引入预热的水中，使得在结晶开始时，温度至少为100 达到C，并且在不高于70℃的温度下将1-萘胺-4,8-​​二磺酸与母液分离。该方法特别有利地用于分离1-萘胺-4,8 来自磺化混合物的二磺酸通过将碱金属硫酸盐，1-萘胺-8-磺酸和SO 3引入到最初引入的硫酸中，总共含有1.5至3摩尔的SO 3和0.6至1.5 每摩尔1-萘胺-8-磺酸使用碱金属硫酸盐的摩尔数。

公开(公告)号：US4369143A

公开(公告)日：1983-01-18

申请号：US287591

申请日：1981-07-28

申请人： Horst Behre ,  Heinz U. Blank ,  Wolfgang Schenk

发明人： Horst Behre ,  Heinz U. Blank ,  Wolfgang Schenk

IPC分类号： C07C309/35 ,  C07C67/00 ,  C07C301/00 ,  C07C303/00 ,  C07C303/06 ,  C07C143/24

CPC分类号： C07C309/00

摘要： A process is provided for the preparation of naphthalene-1,3-5,-trisulphonic acid from 1,5-disulphonated naphthalene, which comprises sulphonating 1,5-disulphonated naphthalene, in the form of a mixture which has been obtained by mixing naphthalene and SO.sub.3 in the presence of an inert solvent at temperatures in the range of -40.degree. to +20.degree. C., the ratio of SO.sub.3 added to naphthalene added having been in the range of 2.5 to 10 mols of SO.sub.3 per mol of naphthalene during the entire addition, at 60.degree. to 110.degree. C. in anhydrous sulphuric acid with oleum, with prior or concurrent separation of the inert solvent.The resulting product is a known intermediate for the formation of azo dyestuffs.

摘要翻译： 提供了从1,5-二磺酸萘制备萘-1,3,5-三磺酸的方法，该方法包括将1,5-二磺酸萘磺化为混合物形式，其通过将萘 和SO 3在惰性溶剂存在下，在-40℃至+ 20℃的温度范围内，加入的萘的添加比例在2.5至10摩尔的SO 3 /摩尔萘的范围内 全部加入，在60〜110℃下用无水硫酸与发烟硫酸，先后或同时分离惰性溶剂。 所得产物是用于形成偶氮染料的已知中间体。

公开(公告)号：US4348336A

公开(公告)日：1982-09-07

申请号：US247414

申请日：1981-03-25

申请人： Heinz U. Blank ,  Horst Behre ,  Hans W. Linden

发明人： Heinz U. Blank ,  Horst Behre ,  Hans W. Linden

IPC分类号： C07C309/47 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C143/60

CPC分类号： C07C303/06

摘要： Process for the isolation of 1-naphthylamine-4,6- or 1-naphthylamine-4,7-disulphonic acid from sulphonation mixtures obtained in the sulphonation of 1-naphthylamine-6- or 1-naphthylamine-7-sulphonic acid with sulphuric acid and sulphur trioxide, wherein the aqueous solutions or suspensions formed, when the sulphonation mixtures are introduced into water, are warmed to 80.degree. to 120.degree. C., optionally kept for a period of time at this temperature, are then cooled to temperatures below 70.degree. C., and the 1-naphthylamine-4,6- or 1-naphthylamine-4,7-disulphonic acid which has crystallized out is finally filtered off.

摘要翻译： 从1-萘胺-6-或1-萘胺-7-磺酸与硫酸磺化得到的磺化混合物中分离1-萘胺-4,6-或1-萘胺-4,7-二磺酸的方法 和三氧化硫，其中当将磺化混合物引入水中时形成的水溶液或悬浮液被加热至80℃至120℃，任选地在该温度下保持一段时间，然后冷却至低于70℃ 并结晶出的1-萘胺-4,6-或1-萘胺-4,7-二磺酸终于被滤出。

公开(公告)号：US4873026A

公开(公告)日：1989-10-10

申请号：US253280

申请日：1988-10-04

申请人： Horst Behre ,  Heinz U. Blank ,  Gerhard Marzolph ,  Willi Streicher

发明人： Horst Behre ,  Heinz U. Blank ,  Gerhard Marzolph ,  Willi Streicher

IPC分类号： C07C301/00 ,  C07C67/00 ,  C07C303/06 ,  C07C309/47

CPC分类号： C07C303/06

摘要： New process for the preparation of 1-aminonaphthalene-2,4,7-trisulphonic acid and, if appropriate, 1,7-Cleve's acid, in which 1-nitronaphthalene is reacted by the Piria method with bisulphites in a manner which is known per se, the sulphamate mixture obtained in this Piria reaction is sulphonated with sulphur trioxide in sulphuric acid to give 1-aminonaphthalene-2,4,7-trisulphonic acid and, if appropriate, this is hydrolysed to 1,7-Cleve's acid by heating in aqueous sulphuric acid.

摘要翻译： 制备1-氨基萘-2,4,7-三磺酸的新方法，如果合适的话，可以将1-硝基萘用Piria法与亚硫酸氢盐反应，如果合适的话，其为1- se，在该Piria反应中得到的氨基磺酸盐混合物用硫酸中的三氧化硫磺化，得到1-氨基萘-2,4,7-三磺酸，如果合适的话，通过加热将其水解成1,7- Cleve酸 硫酸水溶液。

公开(公告)号：US4836959A

公开(公告)日：1989-06-06

申请号：US148478

申请日：1988-01-26

申请人： Willi Streicher ,  Gerhard Marzolph ,  Horst Behre ,  Heinz U. Blank

发明人： Willi Streicher ,  Gerhard Marzolph ,  Horst Behre ,  Heinz U. Blank

IPC分类号： B01J27/055 ,  B01J27/00 ,  B01J27/08 ,  B01J27/18 ,  B01J27/232 ,  B01J31/00 ,  B01J31/02 ,  C07B61/00 ,  C07C303/06 ,  C07C303/22 ,  C07C309/47

CPC分类号： C07C303/06

摘要： The invention relates to a new process for the preparation of 1-aminonaphthalene-2,4,7-trisulphonic acid and 1-aminonaphthalene-7-sulphonic acid (1,7-Cleve's acid), in which 1-aminonaphthalene or naphthionic acid is sulphonated selectively in the presence of certain additives to give 1-aminonaphthalene-2,4,7-trisulphonic acid and this is hydrolyzed to 1,7-Cleve's acid by warming in aqueous sulphuric acid.

摘要翻译： 本发明涉及制备1-氨基萘-2,4,7-三磺酸和1-氨基萘-7-磺酸（1,7-Cleve's acid）的新方法，其中1-氨基萘或萘酸为 在某些添加剂的存在下选择性磺化，得到1-氨基萘-2,4,7-三磺酸，并通过在硫酸水溶液中升温将其水解成1,7-辛二酸。